CN104131284B - A kind of sweep-out method of neodymium-iron-boron permanent magnetic material surface electronickelling - Google Patents
A kind of sweep-out method of neodymium-iron-boron permanent magnetic material surface electronickelling Download PDFInfo
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Abstract
The present invention provides the sweep-out method of a kind of neodymium-iron-boron permanent magnetic material surface electronickelling.The present invention is on the Nd-Fe-B permanent magnet material basis of electroplating surface nickel dam, first carries out oil removing and removing glue with boiling method；The rust on surface is removed with deruster；At room temperature with activating solution, Nd-Fe-B permanent magnet material is carried out activation processing；Using one or both of a nitro paratoluenesulfonic acid sodium salt and m-nitrobenzene sodium sulfonate as main salt chemical reagent, with two kinds in sodium hydride, chlorine water or sodium hydroxide or three kinds for cocatalyst；With one or both in dodecyl sodium sulfate and sodium citrate for stabilizer；And add infiltration liquid make mixed liquor；Adopt sonochemistry method, under the mechanical energy effect of ultrasonic wave concussion, make metal surface nickel dam under main salt chemical reagent and catalytic action, carry out neodymium iron boron and move back nickel chemical treatment.The inventive method is efficient, technique is simple, production cost is low.
Description
Technical field
The present invention relates to the chemical surface treatment field of material, be specifically related to the sweep-out method of a kind of neodymium-iron-boron permanent magnetic material surface electronickelling.
Background technology
Nd-Fe-B permanent magnet material is a kind of magnetic material modern age with good magnetic property, it can pick up the object that object volume is own vol more than 60 times after magnetizing, but it is the element very easily aoxidized owing to Nd-Fe-B permanent magnet material containing the neodymium of about 30%, and Lycoperdon polymorphum Vitt powder is formed on surface, therefore Nd-Fe-B permanent magnet material can not directly make magnetic parts, especially the magnetic sheet of the computer hard disc driver magnet assembly of high-tech area, the magnetic sheet of this magnet assembly requires that its surface must have good overcoat and can be only achieved requirement, current neodymium-iron-boron permanent magnetic material surface is as the coating material of the overcoat of protection, mainly electronickelling, electrogalvanizing etc..Within 1998, U.S.'s US5013411 patent just introduced neodymium iron boron electroplating technology, have employed silicate, drastically increases the viscosity of coating, make binder course firm in this technology.But, in reality high-volume plating Nd-Fe-B permanent magnet material production process, can there is many defect problems in neodymium iron boron product, as plating after neodymium iron boron product in handling process because of the limit arrisdefect that collides with, or cause neodymium iron boron product uneven coating even or pore is bigger etc. owing to electroplating formula or electroplating technology have problems, it is therefore desirable to these are electroplated or the neodymium iron boron product of parcel plating has carried out recycling.
But due to the electroless nickel layer technique that neodymium-iron-boron permanent magnetic material surface is special, frequently resulting in surface nickel dam and do not clean up, product because of the remaining of nonmagnetic nickel element, causes that regeneration Nd-Fe-B permanent magnet material magnetic property is on the low side when again reclaiming (smelting technology).Therefore how to remove the electroless nickel layer of neodymium-iron-boron permanent magnetic material surface efficiently, become the key technical problem of the neodymium iron boron product recycling realizing electroplating nickel on surface.
The purpose of the present invention is precisely in order to overcome and solve the technical problem of above-mentioned existence, on the basis of laboratory work, the sweep-out method of the neodymium-iron-boron permanent magnetic material surface electronickelling of complete set is provided, the demand that high efficiente callback to meet domestic high-volume Nd-Fe-B permanent magnet material recycles, ensures that while reducing production cost reclaiming Nd-Fe-B permanent magnet material product has high-quality and high performance feature.
Summary of the invention
It is an object of the invention to as overcoming the deficiencies in the prior art, it is provided that a kind of efficiently, the sweep-out method of technique is simple, production cost is low neodymium-iron-boron permanent magnetic material surface electronickelling, it is an object of the invention to be achieved through the following technical solutions:
1) oil removing removing glue
A) Nd-Fe-B permanent magnet material carrying out steaming and decocting, temperature controls at 120～200 DEG C, 0.5～3 hour time；
B) being put into by Nd-Fe-B permanent magnet material in removing glue alkali liquor and carry out removing glue, the pH value of removing glue alkali liquor is 8～10.5, and alkali liquid temperature is 60-70 DEG C；
C) carrying out supersound process while steaming and decocting and removing glue, supersonic frequency is 30～80kHz, and power is 200～500w, and the process time is 5～10 minutes；
2) rust cleaning
Remove the rust of neodymium-iron-boron permanent magnetic material surface with deruster, the time is 20～100 seconds, then rinses well with water, and described deruster is the mixed solution of dichloride methane, formic acid, phosphoric acid and infiltration liquid；
3) activation
With activating solution, Nd-Fe-B permanent magnet material being carried out activation processing, under room temperature, soak time is 5～30 seconds, and described activating solution is the mixed liquor of sulfo group acid, table tune powder and infiltration liquid；
4) Nickel Stripping
Nickel Stripping reagent is using a nitro paratoluenesulfonic acid sodium salt and/or m-nitrobenzene sodium sulfonate as main salt chemical reagent, with two or three in sodium hydride, chlorine water and sodium hydroxide for cocatalyst, with dodecyl sodium sulfate and/or sodium citrate for stabilizer, and add infiltration liquid make mixed liquor, pH value is 6.5-7.5, carries out Nickel Stripping process under ul-trasonic irradiation；Described supersonic frequency is 20-80kHz, and power is 50-500W, and temperature is 70-200 DEG C, and the process time is 1-15 minute；
5) post processing
Put in the mixed solution of 10～100ml/l hydrochloric acid l, 10～50ml/l nitric acid and water, at room temperature process 1-5 minute, then rinse well with water.
Preferably, described removing glue alkali liquor formula is sodium carbonate 5～15g/l, sodium phosphate dodecahydrate 10～20g/l, sodium silicate 5～20g/l, OP-10 emulsifying agent 1～5g/l.
Preferably, described deruster formula is dichloride methane 3.5～20g/l, formic acid 5～20g/l, phosphoric acid 5～15g/l, and all the other are infiltration liquid.
Preferably, described activating solution formula is sulfo group acid 10～35g/l, table tune powder 0.5～1.0g/l, and all the other are infiltration liquid.
Preferably, described main salt chemical reagent is nitro paratoluenesulfonic acid sodium salt between 75～100g/l m-nitrobenzene sodium sulfonate and/or 100～120g/l.
Preferably, described cocatalyst is two or three in 75～80g/l sodium hydride, 40～80ml/l chlorine water and 100～150g/l sodium hydroxide.
Preferably, described stabilizer is 0.1～0.5g/l dodecyl sodium sulfate and/or 10～15g/l sodium citrate.
Preferably, described infiltration liquid is ethanol or water.
Preferably, described sweep-out method also includes step baking, is positioned over by the Nd-Fe-B permanent magnet material after post processing in the automatic drying tunnel of Far-infrared Heating and hot air circulation and toasts, and temperature controls at 175～180 DEG C, 1-10 minute time.
Compared with prior art, present invention have the advantage that
1. remove compared with electroless nickel layer or sintering method removal electroless nickel layer with mechanical grinding, the present invention can remove the electroless nickel layer of neodymium-iron-boron permanent magnetic material surface efficiently, cause that the Nd-Fe-B permanent magnet material of regeneration is because of the existence without magnetic nickel element, the recovery product quality obtained is high, magnetic property is good, and product recovery rate is high；And present invention reduces production cost, technical process is simple, easily operates, and is suitable for batch production.
2. the present invention is by controlling the concentration reasonable preparation of main salt chemical reagent, cocatalyst and stability, improve the stability moving back nickel chemical reagent, and control and regulate plating to move back nickel dam speed by optimizing temperature and the process parameter control such as ultrasonic, can removing the electroless nickel layer of neodymium-iron-boron permanent magnetic material surface efficiently, the technological parameter of the present invention is all sum up to draw on the basis of lot of experimental data.
3. removing with mechanical grinding compared with electroless nickel layer or sintering method removal electroless nickel layer, the present invention can obviously reduce oxygen absorbed in neodymium iron boron removal process, is conducive to improving the magnetic property of recycling Nd-Fe-B permanent magnet material；Secondly, the Nickel Stripping method of the present invention can be supplemented, by constantly interpolation, the method consuming ion and be made chemical liquids Reusability, energy-conserving and environment-protective.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
The present invention provides the sweep-out method of a kind of neodymium-iron-boron permanent magnetic material surface electronickelling.The present invention is on the Nd-Fe-B permanent magnet material basis of electroplating surface nickel dam, carries out oil removing and removing glue, and oil removing uses boiling method；The rust on surface is removed with deruster；At room temperature with activating solution, Nd-Fe-B permanent magnet material is carried out activation processing；Using one or both of a nitro paratoluenesulfonic acid sodium salt and m-nitrobenzene sodium sulfonate as main salt chemical reagent, with two kinds in sodium hydride, chlorine water or sodium hydroxide or three kinds for cocatalyst；With one or both in dodecyl sodium sulfate and sodium citrate for stabilizer；And add infiltration liquid make mixed liquor；Adopt sonochemistry method, under the mechanical energy effect of ultrasonic wave concussion, make metal surface nickel dam under main salt chemical reagent and catalytic action, carry out neodymium iron boron and move back nickel chemical treatment.The inventive method is efficient, technique is simple, production cost is low.
The present invention comprises the following steps:
1) oil removing removing glue, first adopt steaming and decocting heat treatment method oil removing, equipment mainly adopts the ultrasonic equipment of precise temperature control, Nd-Fe-B permanent magnet material sample is put in equipped with in the ultrasonic equipment of deionized water, carrying out ultrasonic cooked sample by controlling water temperature, water temperature controls at 120～200 DEG C, and the time is 0.5～3 hour, special concern temperature and time parameter is reasonably combined in operation, it should be noted that prevent from producing the oxidation of neodymium iron boron in steaming and decocting heat treatment process；Then putting into and carry out removing glue in the ultrasonic equipment with alkali liquor, it is 8～10.5 that the pH value of alkali liquor controls, and alkali liquid temperature is 60-70 DEG C；All have employed supersound process while oil removing and removing glue, ultrasonic frequency is 30～80kHz, power is 200～500w, and the process time is 5～10 minutes；Can oil and glue be removed cleaner under hyperacoustic oscillation action.
2) rust cleaning, adopts the mixed liquor of dichloride methane, formic acid, phosphoric acid and infiltration liquid to remove the rust of neodymium-iron-boron permanent magnetic material surface as deruster, and the time is 20～100 seconds, then clean by cold water flush；The deruster of the present invention is gentleer compared with the strong acid abluent such as hydrochloric acid, sulphuric acid, and the pollution of environment is less.
The main chemical reactions equation that may relate in descaling process of the present invention is as follows:
Fe2O3+3H2CO2=6Fe2(CO2)+3H2O
FeO+3H2CO2=FeCO2+3H2O
FeO+H3PO4=Fe (H2PO4)2+H2O；
3) activating, adopt sulfo group acid, table to adjust the mixed liquor of powder and infiltration liquid as activating solution, at room temperature soak time is 5～30 seconds, and the purpose of activation is to make neodymium iron boron surface nickel dam activate, improve its chemical reaction, it is easy to subsequent chemistry moves back the carrying out that nickel processes.The table adopted in the present embodiment adjusts the glue peptide table that powder provides for Xinping, Shenzhen Science and Technology Ltd. to adjust powder, product type LYZ-809, it is mainly composed of titanium salt and keeps additive and pH buffer agent, the water quality survey agent etc. of titanio group activity in solution, product is white size titanium powder regulator, have that adjustment capability is strong, good stability, hard water resistance property are strong, suitable in any water quality and surface of the work before temperature, normal temperature phosphating process, the formation of phosphating coat can be accelerated, making steel surface obtain uniform, fine and closely woven Lycoperdon polymorphum Vitt phosphating coat, phosphating coat has antirust ability strong.
4) Nickel Stripping, Nickel Stripping reagent is using one or both of a nitro paratoluenesulfonic acid sodium salt and m-nitrobenzene sodium sulfonate as main salt chemical reagent, with two or three in sodium hydride, chlorine water and sodium hydroxide for cocatalyst, with one or both in dodecyl sodium sulfate and sodium citrate for stabilizer, and add a certain amount of infiltration liquid and make mixed liquor, pH value is 6.5～7.5, carries out Nickel Stripping process under ultrasonic wave concussion；Ultrasonic technological parameter is as follows: frequency 20～80kHz, power 50～500W, temperature 70～200 DEG C, 1～15 minute time.The main chemical reactions equation that may relate in Nickel Stripping process of the present invention is as follows:
Ni+2H2O=NiO2 -+2H2↑
5) post processing, puts in the mixed solution of 10～100ml/l (unit is ml l) hydrochloric acid, 10～50ml/l nitric acid and water, at room temperature processes 1～5 minute, then clean by cold water flush.Sample surfaces after post processing is bright and clean, without dirt, corrosion-free speckle, sample surfaces metal luster.
Sample after post processing can dry naturally, rate of drying can also be accelerated by baking, in the present embodiment, the Nd-Fe-B permanent magnet material of post processing is positioned in the automatic drying tunnel of Far-infrared Heating and hot air circulation and toast dry, temperature controls at 175～180 DEG C, 1～10 minute time.
In the present embodiment, by the sodium carbonate of 5～15g/l (unit be g/l), the sodium phosphate dodecahydrate of 10～20g/l, the sodium silicate of 5～20g/l, 1～5g/l OP-10 emulsifying agent dissolve, be then configured to removing glue lye solution.
What the present embodiment provided is 3.5～20g/l dichloride methane, 5～20g/l formic acid and 5～15g/l phosphoric acid (concentration of phosphoric acid is 95%) for removing the deruster formula of neodymium-iron-boron permanent magnetic material surface rust.The preparation process of above-mentioned deruster following (to prepare 1L deruster): measure the infiltration liquid of 0.8L, the dichloride methane of 3.5～20g, the formic acid of 5～20g and the phosphoric acid of 5～15g are slowly added into, then add infiltration liquid to 1L, be sufficiently stirred for.
The mixed liquor of powder adjusted by the sulfo group that activating solution formula is 10～35g/l acid and 0.5～1.0g/l table that the present embodiment provides.The preparation process of above-mentioned activating solution following (to prepare 1L activating solution): measure the infiltration liquid of 0.8L, adjusts powder to be slowly added in the table of the acid of the sulfo group of 10～35g and 0.5～1g, then adds infiltration liquid to 1L, is sufficiently stirred for.
In the present embodiment, the preparation process of Nickel Stripping reagent following (to prepare 1L Nickel Stripping reagent): first measure the infiltration liquid of 0.8L, using one or both in nitro paratoluenesulfonic acid sodium salt between 75～100g m-nitrobenzene sodium sulfonate and 100～120g as main salt chemical reagent, by 75～80g sodium hydride, two or more in 40～80ml chlorine water and 100～150g sodium hydroxide is as cocatalyst, using one or both in 0.1～0.5g dodecyl sodium sulfate and 10～15g sodium citrate as stabilizer, it is slowly added into, then infiltration liquid is added to 1L, it is sufficiently stirred for.
In the present embodiment, described infiltration liquid is ethanol or water.
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1
Being put in hot water by the Nd-Fe-B permanent magnet material product of electroplating surface nickel dam steaming and decocting oil removing, temperature controls at 120 DEG C, 3 hours time；Then alkali liquor removing glue is adopted, alkali liquor formula is sodium carbonate: 15g/l, sodium phosphate dodecahydrate: 20g/l, sodium silicate: 20g/l, OP-10 emulsifying agent: 5g/l, pH value controls 10.5, temperature controls at 70 DEG C, adopts frequency to be 80kHz, power be the ultrasonic Treatment 5 minutes of 500w while oil removing and removing glue；It is positioned in deruster by the neodymium iron boron product of oil removing removing glue to remove the rust on surface again, deruster is made up of 3.5g/l dichloride methane, 5g/l formic acid, 5g/l phosphoric acid (concentration of phosphoric acid is 95%) and the mixed liquor of excess water, infiltrating time is 80 seconds, then clean by cold water flush；Then being put in by the neodymium iron boron product handled well in the activating solution being adjusted powder and alcohol blend by the sulfo group acid of 10g/l, 0.5g/l table and carry out activation processing, at room temperature soak time is 30 seconds；
The neodymium iron boron product of surface activation process is positioned in Nickel Stripping reagent and carries out moving back nickel process, Nickel Stripping reagent is using nitro paratoluenesulfonic acid sodium salt mixture between 75g/l m-nitrobenzene sodium sulfonate and 100g/l as main salt, using the mixture of 75g/l sodium hydride, 40ml/l chlorine water and 100g/l sodium hydroxide as cocatalyst, using 0.1g/l dodecyl sodium sulfate and 15g/l sodium citrate as stabilizer, pH value is 7.5, carry out ultrasonic Treatment simultaneously, its parameter is frequency 80kHz, power 100W, temperature 120 DEG C, the process time is 10 minutes；
Then, the neodymium iron boron product that Nickel Stripping processes is put in the mixed solution of 100ml/l hydrochloric acid, 50ml/l nitric acid and water, at room temperature process 1 minute, then clean with cold water wash.
Embodiment 2
Repeat embodiment 1 by described same steps, but Nickel Stripping reagent is using 75g/l m-nitrobenzene sodium sulfonate as main salt, using 75g/l sodium hydride and 40ml/l chlorine water mixture as cocatalyst, using 0.1g/l dodecyl sodium sulfate as stabilizer.Finally, the product after cleaning being placed in the automatic drying tunnel of Far-infrared Heating and hot air circulation and toasted, temperature controls at 175 DEG C, 10 minutes time, namely obtains the recovery neodymium iron boron product that electroplating surface nickel dam has been eliminated completely.
Embodiment 3
Being put in hot water by the Nd-Fe-B permanent magnet material product of electroplating surface nickel dam steaming and decocting oil removing, temperature controls at 200 DEG C, 0.5 hour time；Then alkali liquor removing glue is adopted, alkali liquor formula is sodium carbonate: 5g/l, sodium phosphate dodecahydrate: 10g/l, sodium silicate: 5g/l, OP-10 emulsifying agent: 1g/l, pH value controls 8, temperature controls at 60 DEG C, adopts frequency to be 30kHz, power be the ultrasonic Treatment 10 minutes of 200w while oil removing and removing glue；It is positioned in deruster by the neodymium iron boron product of oil removing removing glue to remove the rust on surface again, deruster is made up of 20g/l dichloride methane, 20g/l formic acid, 15g/l phosphoric acid (concentration of phosphoric acid is 95%) and the mixed liquor of surplus ethanol, infiltrating time is 20 seconds, then clean by cold water flush；Then being put in by the neodymium iron boron product handled well in the activating solution being adjusted powder and alcohol blend by the sulfo group acid of 35g/l, 1.0g/l table and carry out activation processing, at room temperature soak time is 5 seconds；
The neodymium iron boron product of surface activation process is positioned in Nickel Stripping reagent and carries out moving back nickel process, Nickel Stripping reagent is using nitro paratoluenesulfonic acid sodium salt mixture between 100g/l m-nitrobenzene sodium sulfonate and 120g/l as main salt, using the mixture of 80g/l sodium hydride, 80ml/l chlorine water and 150g/l sodium hydroxide as cocatalyst, using 0.3g/l dodecyl sodium sulfate and 10g/l sodium citrate as stabilizer, pH value is 6.5, carry out ultrasonic Treatment simultaneously, its parameter is frequency 20kHz, power 500W, temperature 70 C, the process time is 1 minute；
Then, the neodymium iron boron product that Nickel Stripping processes is put in the mixed solution of 10ml/l hydrochloric acid, 10ml/l nitric acid and water, at room temperature process 5 minutes, then use cold water wash.Finally, the product after cleaning being placed in the automatic drying tunnel of Far-infrared Heating and hot air circulation and toasted, temperature controls at 180 DEG C, 1 minute time, namely obtains the recovery neodymium iron boron product that electroplating surface nickel dam has been eliminated completely.
Embodiment 4
Embodiment 3 is repeated by described same steps, but Nickel Stripping reagent is using nitro paratoluenesulfonic acid sodium salt mixture between 120g/l as main salt, using the mixture of 80ml/l chlorine water and 150g/l sodium hydroxide as cocatalyst, using 10g/l sodium citrate as stabilizer.
Embodiment 5
Being put in hot water by the Nd-Fe-B permanent magnet material product of electroplating surface nickel dam steaming and decocting oil removing, temperature controls at 160 DEG C, 1.5 hours time；Then alkali liquor removing glue is adopted, alkali liquor formula is sodium carbonate: 10g/l, sodium phosphate dodecahydrate: 15g/l, sodium silicate: 15g/l, OP-10 emulsifying agent: 3g/l, pH value controls 9, temperature controls at 65 DEG C, adopts frequency to be 30kHz, power be the ultrasonic Treatment 7 minutes of 400w while oil removing and removing glue；It is positioned in deruster by the neodymium iron boron product of oil removing removing glue to remove the rust on surface again, deruster is made up of 12g/l dichloride methane, 10g/l formic acid, 10g/l phosphoric acid (concentration of phosphoric acid is 95%) and the mixed liquor of excess water, infiltrating time is 100 seconds, then clean by cold water flush；Then being put in by the neodymium iron boron product handled well in the activating solution being adjusted powder and water mixed liquid by the sulfo group acid of 20g/l, 1.0g/l table and carry out activation processing, at room temperature soak time is 20 seconds；
The neodymium iron boron product of surface activation process is positioned in Nickel Stripping reagent and carries out moving back nickel process, Nickel Stripping reagent is using nitro paratoluenesulfonic acid sodium salt mixture between 85g/l m-nitrobenzene sodium sulfonate and 110g/l as main salt, using the mixture of 80g/l sodium hydride, 60ml/l chlorine water and 120g/l sodium hydroxide as cocatalyst, using 0.5g/l dodecyl sodium sulfate and 12g/l sodium citrate as stabilizer, carry out ultrasonic Treatment simultaneously, its parameter is frequency 50kHz, power 50W, temperature 200 DEG C, PH6.5, the process time is 15 minutes；
Then, the neodymium iron boron product that Nickel Stripping processes is put in the mixed solution of 50ml/l hydrochloric acid, 50ml/l nitric acid and water, at room temperature process 3 minutes, then use cold water wash.Finally, the product after cleaning being placed in the automatic drying tunnel of Far-infrared Heating and hot air circulation and toasted, temperature controls at 180 DEG C, 5 minutes time, namely obtains the recovery neodymium iron boron product that electroplating surface nickel dam has been eliminated completely.
Embodiment 6
Repeat embodiment 5 by described same steps, but Nickel Stripping reagent is using 85g/l m-nitrobenzene sodium sulfonate as main salt, using the mixture of 80g/l sodium hydride and 120g/l sodium hydroxide as cocatalyst, using 12g/l sodium citrate as stabilizer.
From the foregoing it can be that the whole technical process of the present invention is simple, production cost is low, it is possible to automatization, easy to operate, and condition controls strict, and an entire flow only needs 2 hours, it can be seen that production capacity is very big, it is possible to fully meet commercial production scale requirement.The present invention can remove the electroless nickel layer of neodymium-iron-boron permanent magnetic material surface efficiently, cause that the neodymium-iron-boron magnetic material of regeneration is because of the existence without magnetic nickel element, the recovery product quality obtained is high, magnetic property is good, product recovery rate is high, it is possible to meet the demand of the high efficiente callback recycling of domestic high-volume neodymium-iron-boron magnetic material.
The present invention is not limited in above-mentioned embodiment, it is impossible to limit the scope of the present invention with this, and the equivalence namely made according to the present patent application the scope of the claims and description changes and modifies, and all should be interpreted that and belongs within the scope that patent of the present invention contains.
Claims (9)
1. the sweep-out method of a neodymium-iron-boron permanent magnetic material surface electronickelling, it is characterised in that comprise the following steps:
1) oil removing removing glue
A) Nd-Fe-B permanent magnet material carrying out steaming and decocting, temperature controls at 120～200 DEG C, 0.5～3 hour time；
B) being put into by Nd-Fe-B permanent magnet material in removing glue alkali liquor and carry out removing glue, the pH value of removing glue alkali liquor is 8～10.5, and alkali liquid temperature is 60-70 DEG C；
C) carrying out supersound process while steaming and decocting and removing glue, supersonic frequency is 30～80kHz, and power is 200～500W, and the process time is 5～10 minutes；
2) rust cleaning
Remove the rust of neodymium-iron-boron permanent magnetic material surface with deruster, the time is 20～100 seconds, then rinses well with water, and described deruster is the mixed solution of dichloride methane, formic acid, phosphoric acid and infiltration liquid；
3) activation
With activating solution, Nd-Fe-B permanent magnet material being carried out activation processing, under room temperature, soak time is 5～30 seconds, and described activating solution is the mixed liquor of sulfo group acid, table tune powder and infiltration liquid；
4) Nickel Stripping
Nickel Stripping reagent is using a nitro paratoluenesulfonic acid sodium salt and/or m-nitrobenzene sodium sulfonate as main salt chemical reagent, with two or three in sodium hydride, chlorine water and sodium hydroxide for cocatalyst, with dodecyl sodium sulfate and/or sodium citrate for stabilizer, and add infiltration liquid make mixed liquor, pH value is 6.5-7.5, carries out Nickel Stripping process under ul-trasonic irradiation；Described supersonic frequency is 20-80kHz, and power is 50-500W, and temperature is 70-200 DEG C, and the process time is 1-15 minute；
5) post processing
Put in the mixed solution of 10～100ml/l hydrochloric acid, 10～50ml/l nitric acid and water, at room temperature process 1-5 minute, then rinse well with water.
2. the sweep-out method of a kind of neodymium-iron-boron permanent magnetic material surface electronickelling according to claim 1, it is characterised in that described removing glue alkali liquor formula is sodium carbonate 5～15g/l, sodium phosphate dodecahydrate 10～20g/l, sodium silicate 5～20g/l, OP-10 emulsifying agent 1～5g/l.
3. the sweep-out method of a kind of neodymium-iron-boron permanent magnetic material surface electronickelling according to claim 1, it is characterised in that described deruster formula is dichloride methane 3.5～20g/l, formic acid 5～20g/l, phosphoric acid 5～15g/l, all the other are infiltration liquid.
4. the sweep-out method of a kind of neodymium-iron-boron permanent magnetic material surface electronickelling according to claim 1, it is characterised in that described activating solution formula is sulfo group acid 10～35g/l, table tune powder 0.5～1.0g/l, and all the other are infiltration liquid.
5. the sweep-out method of a kind of neodymium-iron-boron permanent magnetic material surface electronickelling according to claim 1, it is characterised in that described main salt chemical reagent is nitro paratoluenesulfonic acid sodium salt between 75～100g/l m-nitrobenzene sodium sulfonate and/or 100～120g/l.
6. the sweep-out method of a kind of neodymium-iron-boron permanent magnetic material surface electronickelling according to claim 1, it is characterised in that described cocatalyst is two or three in 75～80g/l sodium hydride, 40～80ml/l chlorine water and 100～150g/l sodium hydroxide.
7. the sweep-out method of a kind of neodymium-iron-boron permanent magnetic material surface electronickelling according to claim 1, it is characterised in that described stabilizer is 0.1～0.5g/l dodecyl sodium sulfate and/or 10～15g/l sodium citrate.
8. the sweep-out method of a kind of neodymium-iron-boron permanent magnetic material surface electronickelling according to any one of claim 1 to 7, it is characterised in that described infiltration liquid is ethanol or water.
9. the sweep-out method of a kind of neodymium-iron-boron permanent magnetic material surface electronickelling according to any one of claim 1 to 7, characterized by further comprising step baking, Nd-Fe-B permanent magnet material after post processing is positioned in the automatic drying tunnel of Far-infrared Heating and hot air circulation and toasts, temperature controls at 175～180 DEG C, 1-10 minute time.
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| CN105149318B (en) * | 2015-08-06 | 2019-02-01 | 安徽大地熊新材料股份有限公司 | A kind of method of nickel plating neodymium iron boron magnetic body removal nickel coating |
| CN105586567B (en) * | 2016-01-04 | 2019-05-14 | 科森科技东台有限公司 | Pre-treatment of vacuum plating processing method |
| CN108435676A (en) * | 2018-02-23 | 2018-08-24 | 廊坊京磁精密材料有限公司 | The glue-removing equipment and method of sintered NdFeB |
| CN113755940B (en) * | 2021-08-26 | 2023-04-14 | 北京航天控制仪器研究所 | Process method for removing electroplated nickel layer on surface of electrical pure iron part |
| CN114395762A (en) * | 2021-12-21 | 2022-04-26 | 宁波韵升股份有限公司 | Method for deplating zinc layer on surface of neodymium-iron-boron magnet |
| CN115999983B (en) * | 2022-08-10 | 2023-08-11 | 宁波十易技术发展有限公司 | Magnetic sheet gumming device |
| CN115537826B (en) * | 2022-09-23 | 2024-08-09 | 安徽省瀚海新材料股份有限公司 | NdFeB multi-wire cooking material oxidation prevention method |
| CN115637333B (en) * | 2022-11-10 | 2023-12-22 | 北京达博有色金属焊料有限责任公司 | Method for recovering metal gold from plated part |
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| JPS54110943A (en) * | 1978-02-20 | 1979-08-30 | Matsushita Electric Ind Co Ltd | Selective stripping liquor for chemical nickel plating |
| CN101775601B (en) * | 2010-02-09 | 2012-05-09 | 合肥工业大学 | Chemical deplating solution and deplating method suitable for removing tin-nickel coating on surface of brass |
| CN101880882B (en) * | 2010-07-01 | 2013-08-07 | 中国科学院宁波材料技术与工程研究所 | Stripping solution for sintered neodymium-iron-boron surface aluminum coating |
| CN103290464B (en) * | 2012-02-24 | 2015-12-02 | 比亚迪股份有限公司 | A kind of electrochemistry removing plating method of stainless steel black film |
| CN102787321B (en) * | 2012-07-30 | 2014-05-14 | 牛凯 | Deplating liquid for NiCuNi plating on surface of sintered NdFeB and deplating process thereof |
| CN102888607B (en) * | 2012-09-24 | 2014-08-06 | 中国人民解放军第五七一九工厂 | Scavenging agent composite for quickly scavenging nickel-cadmium diffusion coating and deplating method of scavenging agent composite |
| CN103160832B (en) * | 2013-04-10 | 2015-06-03 | 四川九洲电器集团有限责任公司 | Stripping solution for chemical nickel-plated coating of cast aluminum piece and stripping method |
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Denomination of invention: Method for removing electroplating nickel on surface of neodymium iron boron permanent magnet material Effective date of registration: 20171018 Granted publication date: 20160713 Pledgee: Industrial Commercial Bank of China Ltd Dongyang branch Pledgor: ZHEJIANG KAIVEN MAGNETIC INDUSTRY CO., LTD. Registration number: 2017330000130 |
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